Research on Zr50Al15−xNi10Cu25Yx amorphous alloys prepared by mechanical alloying with commercial pure element powders

Amorphous Zr₅₀Al_15−xNi₁₀Cu₂₅Y_x alloy powders were fabricated by mechanical alloying at low vacuum with commercial pure element powders. The effects on glass forming ability of Al partial substituted by Y in Zr₅₀Al₁₅Ni₁₀Cu₂₅ and thermal stability of Si₃N₄ powders addition were investigated. The as-milled powders were characterized by X-ray diffraction, scanning electron microscopy and differential scanning calorimeter. The results show that partial substitution of Al can improve the glass forming ability of Zr₅₀Al₁₅Ni₁₀Cu₂₅ alloy. Minor Si₃N₄ additions raise the crystallization activation energy of the amorphous phase and thus improve its thermal stability.     

Crystallization behavior and microstructure of Fe75Co6Zr9B10 alloy

Fe₇₅Co₆Zr₉B₁₀ amorphous alloy prepared by melt-spinning was annealed at various temperatures. The crystallization behavior and microstructure were investigated by differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The three exothermal peaks in the DTA curve of Fe₇₅Co₆Zr₉B₁₀ amorphous alloy correspond to the formations of α-Fe and α-Mn type phases, the growth of BCC-Fe volume fraction at the expense of α-Mn and residual amorphous phase and the precipitations of Fe₃Zr, etc. intermetallic compounds, respectively. The second exothermic peak is not influenced by heating rate, but it shifts to a higher temperature region with increasing preannealing temperature of Fe₇₅Co₆Zr₉B₁₀ alloy. The α-Mn type phase is metastable and its lattice parameter determined by TEM is 0.8830 nm. AFM images show the development of surface morphology of alloy after annealing. The particle size increases with increasing annealing temperature.     

Effect of Zr Addition on Glass-Forming Ability and Magnetic Properties of Fe-Nd-Al-B Alloys Prepared by Suction Casting

The microstructure and magnetic behaviors of the Fe-Nd-Al-B alloys prepared by suction casting with zirconium addition are investigated. With the small amount of zirconium addition, the magnetic properties of the alloys change from hard magnetic property to soft magnetic property. The proper addition of Zr （6%） not only improves the glass forming ability, but also suppresses the crystallization. From the scanning electron microscopy of the [（Fe0.53Nd0.37 Al0.10 ）0.96B0.04]94Zr6 alloy and the local average elemental compositions determined using energy dispersive spectroscopy analysis, the amorphous phase with a composition of Fe47Nd38Al12Zra in the alloy can be observed. The bulk amorphous Fe47Nd38Al12Zr3 alloy is prepared by suction casting exhibiting good glassforming ability and soft magnetic behavior.     

Grain growth process of two-phase nanocrystalline soft magnetic materials

In order to clarify the origin of the high thermal stability of the microstructure in bcc-Fe/amorphous two-phase nanocrystalline soft magnetic materials, we have investigated the changes in the magnetic and microstructural properties upon isothermal annealing at 898 K for an Fe₈₉Zr₇B₃Cu₁ alloy by means of transmission electron microscopy, Mössbauer spectroscopy and DC magnetometry. The mean grain size was found to remain almost unchanged at the early stage of annealing. However, rapid grain coarsening was evident at an annealing time of 7.2 ks where the intergranular amorphous phase begins to crystallize into Fe₂₃Zr₆. The grain growth process with a kinetic exponent of 1.6 is observed for the growth process beyond this annealing time, reflecting the disappearance of the intergranular amorphous phase. Our results confirm that the thermal stability of the bcc-Fe/amorphous two-phase nanocrystalline soft magnetic alloys is governed by the residual amorphous phase.     

具有宽过冷液相区的Fe62Co8-x(Cr,Mo)xNb4Zr6B20非晶态合金的热稳定性与磁性

根据制备块状非晶态合金的三条经验准则,选择了成分为Fe₆₂Co_8-xCr_xNb₄Zr₆B₂₀和Fe₆₂Co_8-xMo_xNb₄Zr₆B₂₀(x=0,2,4)的合金系.利用单辊急冷法制备出厚为30μm宽为5mm左右的条带,并用差热分析、X射线衍射以及 关键词： 过冷液相区 铁磁性 非晶态合金     

Synthesis and magnetic properties of off stoichiometric Laves phase Fe2Nb amorphous alloy

The formation process and magnetic properties of the distorted Laves phase compound (Fe₂Nb) of the nominal composition Fe₆₀Nb₄₀ in its amorphous phase prepared by mechanical alloying have been investigated. The effect of milling time on the formation of amorphous phase has been studied using the X-ray diffraction technique. Further characterizations were carried out by particle size measurement, energy dispersive X-ray microanalysis (EDAX), dc magnetisation and ferromagnetic resonance (FMR) studies. Magnetisation measurement shows that the deviation from the stoichiometric composition in the Nb rich side enhances the compositional short range order and favours the moment formation responsible for weak ferromagnetic behaviour whereas ferromagnetic resonance spectra show some sort of disorder/strain introduced during the mechanical alloying process. The method of preparation also affects the magnetic behaviour of nominal composition Fe₆₀Nb₄₀.     

The effect of Nb addition on the thermal stability and magnetic properties of Fe-based amorphous alloys with a wide supercooled liquid region

We have examined the effect of Nb addition on the thermal stability of the supercooled liquid before crystallization, the glass-forming ability and magnetic properties for the amorphous alloy series Fe₇₃Nb_xAl_5-xGe₂P₁₀C₆B₄ and Fe₆₃Co₇Nb_xZr_10-xB₂₀. The supercooled liquid regions (ΔT_x=T_x-T_g) have maximum values of 66 and 79K, respectively, for Fe₇₃Nb₁Al₄Ge₂P₁₀C₆B₄ and Fe₆₃Co₇Nb₄Zr₆B₂₀ alloys. The saturation magnetization σ_s of the Fe₇₃Nb_xAl_5-xGe₂P₁₀C₆B₄ alloy system is much higher than that of the Fe₆₃Co₇Nb_xZr_10-xB₂₀ alloy system, and is almost unchanged with an increasing Nb content from 0 to 3 at%. But the σ_s of the Fe₆₃Co₇Nb_xZr_10-xB₂₀ alloys decreases linearly with increasing Nb content. The coercive force H_c of the two alloy series can have a minimum value of 31A/m for Fe₇₃Nb₁Al₄Ge₂P₁₀C₆B₄ and 37A/m for Fe₆₃Co₇Nb₄Zr₆B₂₀. All these values are for the ribbons annealed at 773 and 873K for 15min in vacuum.     

Nanocrystalline Fe/Zr alloys: preparation by using mechanical alloying and mechanical milling processes

Nanocrystalline Fe/Zr alloys have been prepared after milling for 9 h the mixture of elemental Fe and Zr powders or the arc-melting produced Fe₂Zr alloy by using mechanical alloying and mechanical milling techniques, respectively. X-ray and Mössbauer results of the Fe and Zr powders, mechanically alloyed, suggest that amorphous Fe₂Zr phase and $\upalpha$ -Fe(Zr) nanograins have been produced with relative concentrations of 91% and 9%, respectively. Conversely, the results of the mechanically milled Fe₂Zr alloy indicate that nanograins of the Fe₂Zr alloy have been formed, surrounded by a magnetic inter-granular phase that are simultaneously dispersed in a paramagnetic amorphous phase.     

NANOSTRUCTURED MULTI-COMPONENT MATERIALS BY MECHANICAL ALLOYING

We have shown that nanostructured multi-component materials like TaC, Nb₇₈Ge₂₂, Mo₇₀Si₂₀B₁₀, Mo₆₀Os₂₀B₂₀, Ru₅₂Zr₆B₄₂, (NbC)₂₀Co₈₀ and (WC)₈₀-(Ti₉₀Cu₁₀)₂₀ with an effective length size reduced to atomic level (a few nanometers) can be produced by mechanical alloying of the elemental and/or alloy powders in a high-energy ball mill. All process steps and samples preparation for characterization were done under glove box conditions.     

The impact of ambient gas on the magnetic properties of Ti40Zr40Ni20 powders during mechanical alloying

Ti₄₀Zr₄₀Ni₂₀ in the form of elemental powders was mechanically alloyed in a planetary ball-mill under argon and hydrogen atmospheres at an acceleration of 55 m s^?2 for different time intervals. The samples were analyzed by X-ray diffraction (XRD), vibrating-sample magnetometry (VSM) and scanning electron microscopy (SEM), which revealed the large impact of the ambient gas, i.e. argon and hydrogen, on the magnetic properties, morphology and structure. Namely, during mechanical alloying in argon the saturation magnetization decreased due to the modification of the Ni d-states upon alloying with paramagnetic Ti and Zr, whereas in hydrogen the Ni d-states remained largely unmodified, since the formation of TiH₂ and ZrH₂ was faster than the alloying with the ferromagnetic nickel. However, after 40 h we obtained a mixture of nanocrystalline Ni and ZrH₂/TiH₂ hydrides, which in equilibrium contained 1.55 mass% of hydrogen. In the case of argon we determined welding of the Ti₄₀Zr₄₀Ni₂₀ amorphous particles, whereas in hydrogen such a process was suppressed by the brittle ZrH₂/TiH₂ hydrides. In addition, we revealed that the mechanical alloying of pure Ni powder for 100 h in argon does not affect its magnetic properties.     

Microstructure and some magnetic properties of bulk amorphous (Fe0.61Co0.10Zr0.025Hf0.025Ti0.02W0.02B0.20)100−xYx (x=0, 2, 3 or 4) alloys

Microstructure, revealed by X-ray diffraction, transmission electron microscopy and Mössbauer spectroscopy, and magnetic properties such as magnetic susceptibility, its disaccommodation, core losses and approach to magnetic saturation in bulk amorphous (Fe_0.61Co_0.10Zr_0.025Hf_0.025Ti_0.02W_0.02B_0.20)_100−xY_x (x=0, 2, 3 or 4) alloys in the as-cast state and after the annealing in vacuum at 720 K for 15 min. are studied. The investigated alloys are ferromagnetic at room temperature. The average hyperfine field induction decreases with Y concentration. Due to annealing out of free volumes its value increases after the heat treatment of the samples. The magnetic susceptibility and core losses point out that the best thermal stability by the amorphous (Fe_0.61Co_0.10Zr_0.025Hf_0.025Ti_0.02W_0.02B_0.20)₉₇Y₃ alloy is exhibited. Moreover, from Mössbauer spectroscopy investigations it is shown that the mentioned above alloy is the most homogeneous. The atom packing density increases with Y concentration, which is proved by the magnetic susceptibility disaccommodation and approach to magnetic saturation studies.     

非晶态Cu56Zr44合金的结构及其等温退火晶化过程的研究

利用X射线衍射技术、差示扫描量热分析技术和透射电子显微镜研究了非晶态Cu₅₆Zr₄₄合金的结构及其等温退火条件下的晶化过程.实验结果表明,非晶态Cu₅₆Zr₄₄合金在室温下的短程结构类似于硬球无规密堆积分布.在703K过冷液相区内等温退火时发现,当退火时间为3min时,晶化产物主要为Cu₈Zr₃相;当退火时间为6min时,Cu₈Zr₃关键词： 非晶态 56Zr₄₄合金')" href="#">Cu₅₆Zr₄₄合金 结构 等温退火     

Thermal stability of Fe3Si-based nanocrystals

We studied the thermal stability of nanocrystalline (Fe₃Si)_0.95Nb_0.05 and Fe₃Si alloys prepared by high-energy ball milling. Alloys were characterized by Mössbauer spectrometry, as well as X-ray diffractometry and transmission electron microscopy. The Nb-containing alloy was considerably more stable against grain growth than was the binary Fe₃Si alloy. Mössbauer spectrometry showed that the Nb atoms segregated away from the DO₃ ordered domains, probably to grain boundaries, and thus provided a strong suppression on grain growth.     

Preparation,microstructure, and magnetic properties of a nanocrystalline Nd12Fe82B6 alloy by HDDR combined with mechanical milling

Nanocrystalline Nd₁₂Fe₈₂B₆ (atomic ratio) alloy powders with Nd₂Fe₁₄B/α-Fe two-phase structure were prepared by HDDR combined with mechanical milling. The as-cast Nd₁₂Fe₈₂B₆ alloy was disproportionated via ball milling in hydrogen, and desorption–recombination was then performed. The phase and structural change due to both the milling in hydrogen and the subsequent desorption–recombination treatment was characterized by X-ray diffraction (XRD). The desorption–recombination behavior of the as-disproportionated alloy was investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The morphology and microstructure of the final alloy powders subject to desorption–recombination treatment were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results showed that, by milling in hydrogen for 20 h, the matrix Nd₂Fe₁₄B phase of the alloy was fully disproportionated into a nano-structured mixture of Nd₂H₅, Fe₂B, and α-Fe phases with average size of about 8 nm, and that a subsequent desorption–recombination treatment at 760 °C for 30 min led to the formation of Nd₂Fe₁₄B/α-Fe two-phase nanocomposite powders with average crystallite size of 30 nm. The remanence B_r, coercivity H_c, and maximum energy product (BH)_max of such nanocrystalline Nd₁₂Fe₈₂B₆ alloy powders achieved 0.73 T, 610 kA/m, and 110.8 kJ/m³, respectively.     

Formation and structure of nanocrystals in bulk Zr<Subscript>50</Subscript>Ti<Subscript>16</Subscript>Cu<Subscript>15</Subscript>Ni<Subscript>19</Subscript> metallic glass

The possible formation of a nanocrystalline structure in controlled crystallization of a bulk Zr₅₀Ti₁₆Cu₁₅Ni₁₉ amorphous alloy has been studied using differential scanning calorimetry, transmission and high-resolution electron microscopy, and x-ray diffraction. It was established that crystallization of the alloy at temperatures above the glass formation point occurs in two stages and brings about the formation of a nanocrystalline structure consisting of three phases. Local spectral x-ray analysis identified the composition and structure of the phases formed.     

Glass-forming ability and thermal stability of Fe<Subscript>62</Subscript>Nb<Subscript>8−x</Subscript>Zr<Subscript>x</Subscript>B<Subscript>30</Subscript> and Fe<Subscript>72</Subscript>Zr<Subscript>8</Subscript>B<Subscript>20</Subscript> amorphous alloys?

Glass-forming ability (GFA) and thermal stability of Fe₆₂Nb₈B₃₀, Fe₆₂Nb₆Zr₂B₃₀ and Fe₇₂Zr₈B₂₀ at % amorphous alloys were investigated by calorimetric (DSC and DTA) measurements. The crystallization kinetics was studied by DSC in the mode of continuous versus linear heating and it was found that both the glass transition temperature, T _g , and the crystallization peak temperature, T _p , display strong dependence on the heating rate. The partial replacement of Nb by Zr leads to lower T _g and T _x temperatures and causes a decrease of the supercooled liquid region. JMA analysis of isothermal transformation data measured between T _g and T _x suggests that the crystallization of the Fe₆₂Nb₈B₃₀ and Fe₆₂Nb₆Zr₂B₃₀ amorphous alloys take place by three-dimensional growth with constant nucleation rate. Nb enhances the precipitation of the metastable Fe₂₃B₆ phase and stabilizes it up to the third crystallization stage. Zr addition increases the lattice constant of Fe₂₃B₆ and, at the same time, decreases the grain size.     

Co-based Soft Magnetic Bulk Materials Prepared by Hot Powder Compaction

Low-coercive bulk amorphous compacts with relative density 99 were prepared by compaction of ball milled Co₅₆Fe₁₆Zr₈B₂₀ ribbons in the supercooled-liquid state. Further, addition of nanocrystalline Fe_72.5Cu₁Nb₂Mo₂Si_15.5B₇ powder to the Co₅₆Fe₁₆Zr₈B₂₀ powder causes a decrease of the magnetostriction of the resultant bulk samples.     

Synthesis and characterization of precipitation hardened amorphous matrix composite by mechanical alloying and pulse plasma sintering of Al65Cu20Ti15

This study reports synthesis of Al₆₅Cu₂₀Ti₁₅ amorphous alloy by mechanical alloying and consolidation of the powder mass by pulsed plasma sintering. During sintering, several intermetallic phases precipitate from the amorphous matrix and cause a significant increase in nano-hardness and elastic modulus. Microstructure in as-milled and sintered conditions was characterized by X-ray diffraction, scanning/transmission electron microscopy and differential scanning calorimetric. Among various conditions of sintering, the composites pulse plasma, sintered at 500°C, show the high compression strength (1745 MPa) and high indentation fracture toughness (4.96 MPa m^1/2); although, the maximum density (3.73 Mg/in³), nano-hardness (14 GPa) and Young's modulus (208 GPa) in the present alloy have been obtained in the composites pulse plasma sintered at 600°C.     

Measurements of the electrical resistance and the hydrogen depth distribution for Ni60Nb20Zr20 amorphous alloy before and after hydrogen charging

A Ni₆₀Nb₂₀Zr₂₀ amorphous alloy was prepared by the single-roller melt-spinning technique. The change in the electrical resistance of the alloy after electrochemical hydrogen charging in 6 N KOH solution was investigated. The change in the hydrogen depth distribution in the alloy was also investigated by elastic recoil detection. As a result, we found that the electrical resistance of the alloy increases with increasing the hydrogen content in the alloy and that a large number of hydrogen atoms are remained in the surface area of the hydrogen-charged alloy.     

Mössbauer effect study on mechanically alloyed amorphous Fe1−x Ti x alloys

Amorphous Fe_1–x Ti _x (x=0.50, 0.60) powders were produced by mechanical alloying from pure elemental powders in a vibratory ball-mill. X-ray diffraction (XRD) and Mössbauer effect (ME) were used to study the progress of amorphization and the property of hydrogen absorption in Fe-Ti alloys. The amorphization process and the properties of the amorphous phase are discussed.